US11511261B2 - Moisture-resistant catalyst for air pollution remediation and method of making the same - Google Patents
Moisture-resistant catalyst for air pollution remediation and method of making the same Download PDFInfo
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- US11511261B2 US11511261B2 US16/825,254 US202016825254A US11511261B2 US 11511261 B2 US11511261 B2 US 11511261B2 US 202016825254 A US202016825254 A US 202016825254A US 11511261 B2 US11511261 B2 US 11511261B2
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- catalyst
- moisture
- sol
- metal oxide
- inorganic
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- 239000003054 catalyst Substances 0.000 title claims abstract description 251
- 238000003915 air pollution Methods 0.000 title claims abstract description 51
- 238000005067 remediation Methods 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 110
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 110
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 46
- 239000013354 porous framework Substances 0.000 claims abstract description 37
- 238000005470 impregnation Methods 0.000 claims abstract description 12
- 230000003100 immobilizing effect Effects 0.000 claims abstract description 7
- 239000004964 aerogel Substances 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 30
- 239000010936 titanium Substances 0.000 claims description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 28
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 28
- 229910052719 titanium Inorganic materials 0.000 claims description 28
- 229910052726 zirconium Inorganic materials 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
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- 229910052735 hafnium Inorganic materials 0.000 claims description 17
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 17
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- YGPLJIIQQIDVFJ-UHFFFAOYSA-N rutherfordium atom Chemical compound [Rf] YGPLJIIQQIDVFJ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052684 Cerium Inorganic materials 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 12
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Definitions
- the disclosure of the present patent application relates to the removal of nitrogen compound pollutants, such as ammonia (NH 3 ), from air, and particularly to a moisture-resistant catalyst for air pollution remediation and, further, to general methods of making moisture-resistant catalysts.
- nitrogen compound pollutants such as ammonia (NH 3 )
- Nitrogen-containing pollutants such as ammonia
- ammonia are not only among the most common of air pollutants, but they are often quite odoriferous. Such odors can be extremely detrimental to the general quality of life, causing not only psychological stress but also physical symptoms, such as insomnia, loss of appetite, etc.
- Nitrogen-containing compounds such as ammonia and organoamines are common sources of odors coming from household food waste, air conditioning systems, garbage dumps, recycling centers, wastewater treatment plants and sewer systems. Such compounds are often generated via the anaerobic decomposition of organic nitrogen-containing waste by microorganisms.
- Ammonia in particular, has a high odor threshold (1.5 ppm), and is known to cause nausea and lung irritation. Exposure to ammonia at very high concentrations can result in permanent lung damage and even death. Ammonia is also toxic to aquatic organisms, especially under conditions of low oxygen concentration. Further, some aromatic amines have been found to be carcinogenic.
- catalytic oxidation process which can significantly decrease the operating temperature of the thermal oxidation process and is a cost-effective method for odor removal.
- catalytic oxidation processes have been difficult to implement on a large scale, due to low catalytic activity under near-ambient conditions and poor selectivity for complete mineralization (i.e., no nitrogen oxide products). It would be desirable to be able to take advantage of the benefits of catalytic oxidation under near-ambient conditions for complete mineralization of ammonia and organoamines.
- a moisture-resistant catalyst for air pollution remediation and a method of making the same solving the aforementioned problems are desired.
- the moisture-resistant catalyst for air pollution remediation is a catalyst with moisture-resistant properties, and which is used for removing nitrogen compound pollutants, such as ammonia (NH 3 ), from air.
- the moisture-resistant catalyst for air pollution remediation includes at least one metal oxide catalyst, at least one inorganic oxide support for supporting the at least one metal oxide catalyst, and a porous framework for immobilizing the at least one metal oxide catalyst and the at least one inorganic oxide support, where the porous framework is moisture-resistant.
- the at least one metal oxide catalyst may be supported on the at least one inorganic oxide support by precipitation, impregnation, dry milling, ion-exchange or combinations thereof.
- the at least one metal oxide catalyst supported on the at least one inorganic oxide support may be physically embedded in the porous framework.
- the moisture-resistant catalyst for air pollution remediation may be used for selective catalytic oxidation of nitrogen-containing compounds into nitrogen, carbon dioxide and water.
- the moisture-resistant catalyst for air pollution remediation may be used to catalyze the oxidation of ammonia in air into nitrogen and water.
- the moisture-resistant catalyst for air pollution remediation may be used to catalyze the oxidation of organoamines in air into nitrogen, carbon dioxide and water. Due to the moisture resistance of the porous framework, the moisture-resistant catalyst for air pollution remediation can be operated at normal operating temperatures at a relative humidity (RH) ranging between 0% and 100%.
- RH relative humidity
- the at least one metal oxide catalyst may be an oxide from Group IB (copper, silver or gold), Group IIB (zinc, cadmium or mercury), Group IIIB (scandium, yttrium, lanthanum or cerium), Group IVB (titanium, zirconium, hafnium or rutherfordium), Group VB (vanadium, niobium, tantalum or dubnium), Group VIB (chromium, molybdenum, tungsten or seaborgium), Group VIIB (manganese, technetium, rhenium or bohrium), Group VIIIB (iron, ruthenium, osmium, hassium, cobalt, rhodium, iridium, meitnerium, nickel, palladium, platinum or darmstadtium) or combinations thereof.
- Group IB copper, silver or gold
- Group IIB zinc, cadmium or mercury
- Group IIIB scandium, yttrium, lanthanum
- the at least one metal oxide catalyst may be an oxide of copper, zinc, yttrium, lanthanum, cerium, titanium, zirconium, vanadium, chromium, manganese, iron, cobalt, nickel or combinations thereof.
- the at least one inorganic oxide support may be an oxide from Group IIIA (aluminum, gallium, indium, thallium or nihonium), Group IVA (silicon, germanium, tin, lead or flerovium), Group IVB (titanium, zirconium, hafnium or rutherfordium) or combinations thereof.
- the at least one inorganic oxide support may be an oxide of aluminum, silicon, titanium, zirconium or combinations thereof.
- the porous framework prevents penetration of water droplets and moisture, and may be a hydrophobic material for repelling the water droplets and moisture.
- the porous framework may also have relatively narrow pores, which surround the catalyst, for preventing penetration by the water droplets and moisture.
- the porous framework may be an inorganic aerogel, for example, a silica aerogel, a titania-silica aerogel, a silicon nitride aerogel, a graphene aerogel, a carbon aerogel or an aerogel formed from carbonaceous materials that exhibit intrinsic hydrophobic properties or are modified or functionalized to exhibt hydrophobic properties.
- the modification and/or functionalization may involve the use of silanes, such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- silanes such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- the porous framework may be a porous polymer matrix formed from at least one hydrophobic polymer, for example, polyacrylates, polyamides, polycarbonates, polyfluorocarbons, polystyrenes, polyimides, resorcinol-formaldehyde polymers or combinations thereof.
- the porous framework may be a mixed inorganic and organic matrix, including at least one hydrophobic polymer and at least one inorganic component, for example, silica, titania-silica, silicon nitride, graphene, carbon or carbonaceous materials that exhibit intrinsic hydrophobic properties or are modified or functionalized to exhibt hydrophobic properties.
- the modification and/or functionalization may involve the use of silanes, such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- silanes such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- the moisture-resistant catalyst for air pollution remediation may also include a promoter, for example, a promoter belonging to Group IVB (titanium, zirconium, hafnium or rutherfordium), Group VB (vanadium, niobium, tantalum or dubnium) or combinations thereof. Additionally, the moisture-resistant catalyst for air pollution remediation may also include a stabilizer, for example, a stabilizer belonging to Group IIIA (boron, aluminum, gallium, indium, thallium or nihonium), Group IVA (carbon, silicon, germanium, tin, lead or flerovium), Group IVB (titanium, zirconium, hafnium or rutherfordium) or combinations thereof.
- a promoter for example, a promoter belonging to Group IVB (titanium, zirconium, hafnium or rutherfordium), Group VB (vanadium, niobium, tantalum or dubnium) or combinations thereof.
- the moisture-resistant catalyst for air pollution remediation may also include an inhibitor, for example, an inhibitor belonging to Group IB (copper, silver or gold), Group IIIB (scandium, yttrium, lanthanum or cerium), Group VIIIB (iron, ruthenium, osmium, hassium, cobalt, rhodium, iridium, meitnerium, nickel, palladium, platinum or darmstadtium) or combinations thereof.
- an inhibitor for example, an inhibitor belonging to Group IB (copper, silver or gold), Group IIIB (scandium, yttrium, lanthanum or cerium), Group VIIIB (iron, ruthenium, osmium, hassium, cobalt, rhodium, iridium, meitnerium, nickel, palladium, platinum or darmstadtium) or combinations thereof.
- the moisture-resistant catalyst for air pollution remediation may be made using a one-pot synthesis method.
- the at least one metal oxide catalyst and the at least one inorganic oxide support are initially dispersed into a sol, which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a sol which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a condensation agent or a crosslinking agent is then added to the sol with the added catalyst to produce a catalyst-containing gel.
- the particular sol-gel process for producing the catalyst-containing gel is dependent upon whether the sol is an inorganic sol, an organic sol or an inorganic-organic hybrid sol.
- the moisture-resistant catalyst is then obtained through drying (e.g., supercritical drying, freeze drying, conventional drying or the like) and an appropriate thermal treatment processes to remove water and solvents within the catalyst-containing gel.
- the moisture-resistant catalyst for air pollution remediation may be made using an impregnation method, where the at least one metal oxide catalyst is immobilized on the at least one inorganic oxide support.
- the at least one inorganic oxide support is initially dispersed into a sol, which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a sol which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a condensation agent or a crosslinking agent is then added to the sol with the added support to produce a support-containing gel.
- the particular sol-gel process for producing the support-containing gel is dependent upon whether the sol is an inorganic sol, an organic sol or an inorganic-organic hybrid sol.
- the support-containing gel is then dried (e.g., supercritical drying, freeze drying, conventional drying or the like) to form a support-containing aerogel, and the at least one metal oxide catalyst is then immobilized on the support-containing aerogel through conventional impregnation. Further drying and appropriate thermal treatment process(es) are then applied to produce the moisture-resistant catalyst.
- This impregnation-based method can avoid the adverse effect of complex synthesis systems to prepare the moisture-resistant catalyst with more accessible catalytic active sites.
- the moisture-resistant catalyst for air pollution remediation may be made using mixing combined with catalyst surface modification.
- the at least one metal oxide catalyst is initially dispersed into a sol, which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a sol e.g., metal oxides, graphene derivatives or the like
- an organic sol e.g., polymers
- an inorganic-organic hybrid sol e.g., silicone, a metal oxide-polymer or the like.
- a condensation agent or a crosslinking agent is then added to the sol with the added catalyst to produce a catalyst-containing gel.
- the particular sol-gel process for producing the catalyst-containing gel is dependent upon whether the sol is an inorganic sol, an organic sol or an inorganic-organic hybrid sol.
- FIG. 1 is a graph comparing nitrogen adsorption/desorption isotherms of conventional silica aerogel, a conventional metal oxide catalyst, and a moisture-resistant catalyst for air pollution remediation.
- FIG. 2A is graph showing mesopore size distribution of the conventional silica aerogel.
- FIG. 2B is graph showing mesopore size distribution of the moisture-resistant catalyst for air pollution remediation.
- FIG. 3 is a graph showing ammonia (NH 3 ) concentration as a function of time for the conventional metal oxide catalyst (shown for two different loadings of the catalyst) at room temperature under dry conditions.
- FIG. 4 is a graph showing ammonia (NH 3 ) conversion as a function of temperature for the conventional metal oxide catalyst under a relative humidity of 100%.
- FIG. 5 is a graph comparing reaction rates of ammonia (NH 3 ) oxidation for the conventional metal oxide catalyst (shown as “Catalyst 1”) under 0% relative humidity (RH) and 100% RH and the moisture-resistant catalyst for air pollution remediation (shown as “Catalyst 2”) under 0% RH and 100% RH.
- NH 3 ammonia
- FIG. 6 is a graph comparing reaction rates of ammonia (NH 3 ) oxidation and nitrogen selectivity for the conventional metal oxide catalyst at inhibitor loadings of 10% and 30% at varying temperatures under dry conditions.
- FIG. 7 is a graph comparing reaction rates of ammonia (NH 3 ) oxidation for the conventional metal oxide catalyst with promoters and without promoters at varying temperatures under dry conditions.
- FIG. 8 is a graph comparing reaction rates of ammonia (NH 3 ) oxidation for the conventional metal oxide catalyst (shown as “Catalyst 1”) with promoters under 0% relative humidity (RH) and 100% RH and the moisture-resistant catalyst for air pollution remediation (shown as “Catalyst 2”) under 0% RH and 100% RH at varying temperatures.
- NH 3 ammonia
- FIG. 9A schematically illustrates a one-pot synthesis-based method for making the moisture-resistant catalyst for air pollution remediation.
- FIG. 9B schematically illustrates an impregnation-based method for making the moisture-resistant catalyst for air pollution remediation.
- FIG. 9C schematically illustrates a physical mixing-based method for making the moisture-resistant catalyst for air pollution remediation.
- FIG. 10A illustrates a conventional sol-gel reaction for the formation of an inorganic gel.
- FIG. 10B illustrates a conventional sol-gel reaction for the formation of an organic gel.
- FIG. 10C illustrates a conventional sol-gel reaction for the formation of an inorganic-organic hybrid gel.
- the moisture-resistant catalyst for air pollution remediation is a catalyst with moisture-resistant properties, and which is used for removing nitrogen compound pollutants, such as ammonia (NH 3 ), from air.
- the moisture-resistant catalyst for air pollution remediation includes at least one metal oxide catalyst, at least one inorganic oxide support for supporting the at least one metal oxide catalyst, and a porous framework for the at least one metal oxide catalyst and the at least one inorganic oxide support, where the porous framework is moisture-resistant.
- the at least one metal oxide catalyst may be supported on the at least one inorganic oxide support by precipitation, impregnation, dry milling, ion-exchange or combinations thereof.
- the at least one metal oxide catalyst supported on the at least one inorganic oxide support may be physically embedded in the porous framework.
- the moisture-resistant catalyst for air pollution remediation may be used for selective catalytic oxidation of nitrogen-containing compounds into nitrogen, carbon dioxide and water.
- the moisture-resistant catalyst for air pollution remediation may be used to catalyze the oxidation of ammonia in air into nitrogen and water.
- the moisture-resistant catalyst for air pollution remediation may be used to catalyze the oxidation of organoamines in air into nitrogen, carbon dioxide and water. Due to the moisture resistance of the porous framework, the moisture-resistant catalyst for air pollution remediation can operate at normal operating temperatures at a relative humidity (RH) ranging between 0% and 100%.
- RH relative humidity
- the at least one metal oxide catalyst may be an oxide from Group IB (copper, silver or gold), Group IIB (zinc, cadmium or mercury), Group IIIB (scandium, yttrium, lanthanum or cerium), Group IVB (titanium, zirconium, hafnium or rutherfordium), Group VB (vanadium, niobium, tantalum or dubnium), Group VIB (chromium, molybdenum, tungsten or seaborgium), Group VIIB (manganese, technetium, rhenium or bohrium), Group VIIIB (iron, ruthenium, osmium, hassium, cobalt, rhodium, iridium, meitnerium, nickel, palladium, platinum or darmstadtium) or combinations thereof.
- Group IB copper, silver or gold
- Group IIB zinc, cadmium or mercury
- Group IIIB scandium, yttrium, lanthanum
- the at least one metal oxide catalyst may be an oxide of copper, zinc, yttrium, lanthanum, cerium, titanium, zirconium, vanadium, chromium, manganese, iron, cobalt, nickel or combinations thereof.
- the at least one inorganic oxide support may be an oxide from Group IIIA (aluminum, gallium, indium, thallium or nihonium), Group IVA (silicon, germanium, tin, lead or flerovium), Group IVB (titanium, zirconium, hafnium or rutherfordium) or combinations thereof.
- the at least one inorganic oxide support may be an oxide of aluminum, silicon, titanium, zirconium or combinations thereof.
- the porous framework prevents penetration of water droplets and moisture, and may be a hydrophobic material for repelling the water droplets and moisture.
- the porous framework may also have relatively narrow pores, which surround the catalyst, for preventing penetration by the water droplets and moisture.
- the porous framework may be an inorganic aerogel, for example, a silica aerogel, a titania-silica aerogel, a silicon nitride aerogel, a graphene aerogel, a carbon aerogel or an aerogel formed from carbonaceous materials that exhibit intrinsic hydrophobic properties or are modified or functionalized to exhibt hydrophobic properties.
- the modification and/or functionalization may involve the use of silanes, such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- silanes such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- the porous framework may be a porous polymer matrix formed from at least one hydrophobic polymer, for example, polyacrylates, polyamides, polycarbonates, polyfluorocarbons, polystyrenes, polyimides, resorcinol-formaldehyde polymers or combinations thereof.
- the porous framework may be a mixed inorganic and organic matrix, including at least one hydrophobic polymer and at least one inorganic component, for example, silica, titania-silica, silicon nitride, graphene, carbon or carbonaceous materials that exhibit intrinsic hydrophobic properties or are modified or functionalized to exhibt hydrophobic properties.
- the modification and/or functionalization may involve the use of silanes, such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- silanes such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, or hexamethyldisilazane.
- the moisture-resistant catalyst for air pollution remediation may also include a promoter, for example, a promoter belonging to Group IVB (titanium, zirconium, hafnium or rutherfordium), Group VB (vanadium, niobium, tantalum or dubnium) or combinations thereof. Additionally, the moisture-resistant catalyst for air pollution remediation may also include a stabilizer, for example, a stabilizer belonging to Group IIIA (boron, aluminum, gallium, indium, thallium or nihonium), Group IVA (carbon, silicon, germanium, tin, lead or flerovium), Group IVB (titanium, zirconium, hafnium or rutherfordium) or combinations thereof.
- a promoter for example, a promoter belonging to Group IVB (titanium, zirconium, hafnium or rutherfordium), Group VB (vanadium, niobium, tantalum or dubnium) or combinations thereof.
- the moisture-resistant catalyst for air pollution remediation may also include an inhibitor, for example, an inhibitor belonging to Group IB (copper, silver or gold), Group IIIB (scandium, yttrium, lanthanum or cerium), Group VIIIB (iron, ruthenium, osmium, hassium, cobalt, rhodium, iridium, meitnerium, nickel, palladium, platinum or darmstadtium) or combinations thereof.
- an inhibitor for example, an inhibitor belonging to Group IB (copper, silver or gold), Group IIIB (scandium, yttrium, lanthanum or cerium), Group VIIIB (iron, ruthenium, osmium, hassium, cobalt, rhodium, iridium, meitnerium, nickel, palladium, platinum or darmstadtium) or combinations thereof.
- the moisture-resistant catalyst for air pollution remediation may be made using a one-pot synthesis method.
- the at least one metal oxide catalyst and the at least one inorganic oxide support are initially dispersed into a sol, which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a sol which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a condensation agent or a crosslinking agent is then added to the sol with the added catalyst to produce a catalyst-containing gel.
- the particular sol-gel process for producing the catalyst-containing gel is dependent upon whether the sol is an inorganic sol, an organic sol or an inorganic-organic hybrid sol.
- the moisture-resistant catalyst is then obtained through drying (e.g., supercritical drying, freeze drying, conventional drying or the like) and an appropriate thermal treatment processes to remove water and solvents within the catalyst-containing gel.
- the moisture-resistant catalyst for air pollution remediation may be made using an impregnation method, where the at least one metal oxide catalyst is immobilized on the at least one inorganic oxide support.
- the at least one inorganic oxide support is initially dispersed into a sol, which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a sol which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a condensation agent or a crosslinking agent is then added to the sol with the added support to produce a support-containing gel.
- the particular sol-gel process for producing the support-containing gel is dependent upon whether the sol is an inorganic sol, an organic sol or an inorganic-organic hybrid sol.
- the support-containing gel is then dried (e.g., supercritical drying, freeze drying, conventional drying or the like) to form a support-containing aerogel, and the at least one metal oxide catalyst is then immobilized on the support-containing aerogel through conventional impregnation. Further drying and appropriate thermal treatment process(es) are then applied to produce the moisture-resistant catalyst.
- This impregnation-based method can avoid the adverse effect of complex synthesis systems to prepare the moisture-resistant catalyst with more accessible catalytic active sites.
- the moisture-resistant catalyst for air pollution remediation may be made using mixing combined with catalyst surface modification.
- the at least one metal oxide catalyst is initially dispersed into a sol, which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a sol which may be an inorganic sol (e.g., metal oxides, graphene derivatives or the like), an organic sol (e.g., polymers), or an inorganic-organic hybrid sol (e.g., silicone, a metal oxide-polymer or the like).
- a condensation agent or a crosslinking agent is then added to the sol with the added catalyst to produce a catalyst-containing gel.
- the particular sol-gel process for producing the catalyst-containing gel is dependent upon whether the sol is an inorganic sol, an organic sol or an inorganic-organic hybrid sol.
- the moisture-resistant catalyst is then obtained through drying (e.g., supercritical drying, freeze drying, conventional drying or the like) and an appropriate thermal treatment processes to remove water and solvents within the catalyst-containing gel.
- the sol-gel processes may be any suitable type of conventional sol-gel processes, as would be well known to one having ordinary skill in the art.
- FIG. 10A illustrates a conventional sol-gel process for the formation of an inorganic gel.
- FIG. 10B illustrates a conventional sol-gel process for the formation of an organic gel.
- FIG. 10C illustrates a conventional sol-gel process for the formation of an inorganic-organic hybrid gel.
- Conventional metal oxide sols such as silica sol, titania sol or the like, may be prepared from metal alkoxides through hydrolysis and condensation processes catalyzed by acids or bases.
- the condensation process finally leads to solidification of sol systems to form metal oxide gels with crosslinked networks.
- the condensation process of water-soluble metal salts and colloidal metal oxides is induced by acids or bases to form colloidal metal oxide gels.
- the sol-gel chemistry of the organic gel is generally based on the polymerization of monomers in the presence of initiators and crosslinkers.
- Metal oxide sols prepared from metal alkoxides can be further crosslinked with organic ligands to form inorganic-organic hybrid gels.
- a typical example is a silicone-based inorganic-organic hybrid gel.
- Another typical example is an inorganic-organic hybrid gel with bi-continuous gel networks evolved from physically mixed an inorganic sol and an organic sol.
- Examples 1-7 below describe the production of various sols
- examples 8-17 below describe the production of various aerogels
- examples 18-21 below describe the production of conventional plain metal oxide catalysts
- examples 22-24 below describe the production of the present moisture-resistant catalysts
- examples 25 and 26 describe experiments for testing catalytic reactions under dry and wet conditions, respectively.
- FIG. 1 shows the nitrogen adsorption/desorption isotherms of plain silica aerogel, a plain metal oxide catalyst and the present moisture-resistant catalyst, prepared as described above. Table 1 below lists their specific surface area and pore structure data obtained from the isotherms.
- the plain metal oxide catalyst exhibits the lowest specific surface area from intercrystalline pores.
- the silica aerogel and the moisture-resistant catalyst have typical mesoporous structures, indicated by hysteresis loops in their isotherms. They also contain some micropores. The total pore volumes of the silica aerogel and the moisture-resistant catalyst are more than 9 times of that of the initial metal oxide catalyst.
- FIG. 2A shows the mesopore size distribution of the silica aerogel
- FIG. 2B shows the mesopore size distribution of the moisture-resistant catalyst. As shown, they have uniform mesopore size distributions centralized at 13 nm and 7 nm, respectively.
- FIG. 3 shows NH 3 concentration vs. time curves of the plain metal oxide catalyst at room temperature and under dry conditions.
- the metal oxide catalyst (25 mg) is able to convert NH 3 at more than 50% conversion for 40 ppm NH 3 in 400 ml/min of air at room temperature.
- 90% NH 3 conversion was reached to lower the ammonia concentration near the odor threshold.
- FIG. 5 shows a comparison of the catalytic reaction rates of NH 3 oxidation on the plain metal oxide catalysts and corresponding moisture-resistant catalysts under different conditions.
- FIG. 6 compares the catalytic reaction rates of NH 3 oxidation and nitrogen selectivities on the plain metal oxide catalysts with different inhibitor loadings. With the increase of inhibitor loading, the catalytic activities of the metal oxide catalysts at low temperatures are remarkably improved. High inhibitor loading also avoids the deep oxidation of NH 3 to form nitrogen oxide products.
- FIG. 7 compares the catalytic reaction rates of NH 3 oxidation on the metal oxide catalysts without and with promoters at different temperatures. The promoters significantly enhance catalytic activities of the metal oxide catalyst in the full range of operating temperatures.
- FIG. 8 shows the catalytic reaction rates of NH 3 oxidation on the metal oxide catalysts with promoters and the corresponding moisture-resistant catalysts under different temperatures and relative humidities. The moisture-resistant catalysts exhibit much higher catalytic activities than the metal oxide catalyst with promoters. Relative humidity is shown not to affect the catalytic activities of the moisture-resistant catalysts.
- Silica sol was prepared by adding diluted nitric acid (0.14 mol/l, 9.6 ml) to tetraethyl orthosilicate (30 ml) under stirring, followed by heating at 50° C. for 3 hours to obtain a clear silica sol.
- Alumina sol was prepared by dispersing commercial pseudoboehmite powder (3.4 g) into DDI water (47 ml) under vigorous stirring, followed by heating at 80° C. and adding diluted nitric acid (1.6 mol/l, 1.8 ml). The obtained mixture was further stirred at 80° C. for 6 hours to obtain a clear alumina sol (1 mol/l).
- a titania sol was prepared by dissolving titanium isopropoxide (10 ml) in isopropanol (23.6 ml), followed by adding HNO 3 (2 mol/l, 3.4 ml) and DDI water (31.4 ml) under vigorous stirring to obtain an opaque suspension. The suspension was further stirred at 80° C. to evaporate isopropanol and peptizing titania precipitate, followed by cooling down to room temperature and stirring overnight to obtain a clear titania sol (1 mol/l).
- Zirconia sol was prepared by dissolving zirconium isopropoxide (11 g) in isopropanol (23.6 ml), followed by adding HNO 3 (2 mol/l, 3.4 ml) and DDI water (31.4 ml) under vigorous stirring to obtain an opaque suspension. The suspension was further stirred at 80° C. to evaporate isopropanol and peptizing zirconia precipitate, followed by cooling down to room temperature and stirring overnight to obtain a clear zirconia sol (1 mol/l).
- a silica-alumina sol was prepared by adding tetraethyl orthosilicate (22 ml) to acidic boehmite sol (0.2 mol/l, 50 ml) under vigorous stirring, followed by stirring for 24 hours at room temperature to form a clear silica-alumina sol with a Si/Al ratio of 10.
- a silica-titania sol was prepared by adding tetraethyl orthosilicate (22 ml) to titania sol (1 mol/l, 50 ml) under vigorous stirring, followed by stirring for 24 hours at room temperature to form a clear silica-titania sol with a Si/Ti ratio of 2.
- a silica-zirconia sol was prepared by adding tetraethyl orthosilicate (22 ml) to zirconia sol (0.2 mol/l, 50 ml) under vigorous stirring, followed by stirring for 24 hours at room temperature to form a clear silica-zirconia sol with a Si/Zr ratio of 10.
- a silica aerogel was formed by adding weak basic reagents, including sodium carbonate solution, ammonia solution and a colloidal silica dispersion, to an acidic silica sol to induce a slow condensation process for silica gel formation.
- the gelation time is adjustable by concentration and the amount of weak basic reagents to form gel networks with monolithic morphology and enough mechanical strength. It should be noted that a too rapid or too slow gelation process results in the precipitation of silica sol or soft gel networks. Water and solvents of silica gel were removed by supercritical drying (or freeze drying) and further thermal treatment under different atmospheres to obtain a silica aerogel.
- the silica aerogel can be further functionalized with silanes, such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane or hexamethyldisilazane to increase its hydrophobicity.
- silanes such as methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane or hexamethyldisilazane to increase its hydrophobicity.
- a silica-alumina aerogel was prepared from the silica-alumina sol of Example 5 by similar processes of base-induced condensation, drying and thermal treatment according to that described in Example 8.
- a silica-titania aerogel was prepared from the silica-titania sol of Example 6 by similar processes of base-induced condensation, drying and thermal treatment according to that described in Example 8.
- a silica-zirconia aerogel was prepared from the silica-zirconia sol of Example 7 by similar processes of base-induced condensation, drying and thermal treatment according to those described in Example 8.
- a graphene aerogel was prepared from graphene oxide nanosheets, which were made using a modified Hummers method, and which were dispersed in DDI water with a concentration range of 1-10 mg/ml, followed by adding crosslinkers containing amino groups, such as ethylenediamine and polyethylenimine.
- the obtained suspension was hydrothermal-treated through a conventional oven or a microwave oven to prepare a graphene gel.
- the graphene aerogel was prepared from the graphene gel by supercritical drying or freeze drying.
- a resorcinol-formaldehyde aerogel was prepared by dissolving resorcinol and formaldehyde, with molar ratio of 1:2, in DDI water, followed by adding sodium carbonate solution and heating at 85° C. for several days to obtain the resorcinol-formaldehyde gel.
- the gel was placed into an acetic acid solution (5%) to increase the crosslinking density of gel networks. Finally, a supercritical drying process was carried out to obtain the resorcinol-formaldehyde aerogel.
- a polymer aerogel was prepared from polymer gels, which were made through a polymerization process of monomers in the presence of initiators and crosslinkers.
- biphenyl-3,3′,4,4′-tetracarboxylic diandride (4.8 g) and 4,4′-oxydianiline (3.2 g) were dissolved in N-methylpyrrolidinone (50 ml), followed by adding 1,3,5-triaminophenoxybenzene solution in N-methylpyrrolidinone (0.2 g in 16 ml) under stirring. Then, acetic anhydride (12.3 ml) and pyridine (10.5 ml) were added to the above solution to obtain a polyimide gel. The obtained polyimide gel was further aged for 24 hours, followed by solvent exchange and supercritical drying to obtain the polyimide aerogel.
- Carbonaceous and carbon aerogels were prepared by carbonizing the resorcinol-formaldehyde aerogel of Example 13, or other polymer aerogels, at low and high temperatures and in inert atmospheres, respectively.
- Inorganic-organic aerogels with a single network were prepared from inorganic-organic gels with a single network.
- the inorganic-organic gels with a single network were prepared by a co-condensation process of metal alkoxides and corresponding organic ligands.
- methyltriethoxysilane 5.4 ml was dissolved in malonic acid aqueous solution (0.1%, 10 ml), followed by adding glucose (1 g) and dimethoxydimethylsilane (2.2 ml) under stirring.
- Urea (4 g) and cetyltrimethylammonium chloride (1 g) was added into the above solution under stirring to obtain a silicone-based inorganic-organic sol.
- a silicone-based inorganic-organic gel was prepared by heating the sol at 75° C. for 4 hours, followed by drying at 120° C. to obtain the silicone-based inorganic-organic aerogel.
- Inorganic-organic aerogels with bi-continuous networks were prepared from inorganic-organic gels with bi-continuous networks.
- the inorganic-organic gels with bi-continuous networks were prepared by mixing metal oxide sols (described above in Examples 1-7) or a graphene oxide dispersion (described in Example 12) and resorcinol-formaldehyde or monomer solutions (described in Examples 13 and 14) and adjusting their gelation processes with condensation agents and crosslinkers.
- Inorganic-organic aerogels with bi-continuous networks were obtained after solvent exchange and supercritical drying processes.
- Metal oxide catalysts were prepared by supporting active components selected from Group IB, IIB, IIIB, IVB, VB, VIB, VIIB and VIIIB elements on metal oxide supports selected from Group IIIA, IVA and IVB elements.
- a typical example is a vanadium oxide catalyst supported on titania.
- Ammonium metavanadate (0.1 g) was dissolved in DDI water (50 ml) under vigorous stirring, followed by adding a titania support (0.5 g). The obtained suspension was dried at 60° C. using a rotary evaporator under vacuum, and further dried at 120° C. for 24 hours and calcined at 250° C. in air for 6 hours to obtain a VO x /TiO 2 catalyst.
- Metal oxide catalysts with promoters were prepared using promoters selected from Group IVB and VB elements, which were added into an active component aqueous solution to prepare the metal oxide catalysts with promoters for enhanced catalytic activity.
- the process used was similar to the procedure given above in Example 18.
- zirconium oxynitrate hydrate (0.1 g) and ammonium metavanadate (0.1 g) were dissolved in DDI water (50 ml) under vigorous stirring, followed by adding a titania support (0.5 g).
- the obtained suspension was dried at 60° C. using a rotary evaporator under vacuum, and further dried at 120° C. for 24 hours and calcined at 400° C. in air for 6 hours to obtain a ZrO 2 —VO x /TiO 2 catalyst.
- Metal oxide catalysts with inhibitors were prepared using inhibitors selected from Group IB, IIIB and VIIIB elements, which were added into the active component aqueous solution to prepare metal oxide catalysts with inhibitors for improved catalytic selectivity.
- the process used was similar to that described above in Example 18.
- copper nitrate trihydrate (0.45 g) and ammonium metavanadate (0.1 g) were dissolved in DDI water (50 ml) under vigorous stirring, followed by adding a titania support (0.5 g).
- the obtained suspension was dried at 60° C. using a rotary evaporator under vacuum, and further dried at 120° C. for 24 hours and calcined at 400° C. in air for 6 hours to obtain a CuO—VO x /TiO 2 catalyst.
- Metal oxide catalysts with stabilizers were prepared using stabilizers selected from Group IIIA, IVA and IVB elements, which were added to the active component aqueous solution to prepare metal oxide catalysts with stabilizers for improved catalyst stability.
- the process used was similar to that described above in Example 18.
- ammonium metavanadate (0.1 g) was dissolved in DDI water (50 ml) under vigorous stirring, followed by adding a titania support (0.4 g) and a colloidal silica stabilizer suspension (40%, 0.13 g).
- the obtained suspension was dried at 60° C. using a rotary evaporator under vacuum, and further dried at 120° C. for 24 hours and calcined at 400° C. in air for 6 hours to obtain a VO x /SiO 2 —TiO 2 catalyst.
- the moisture-resistant catalyst was prepared using catalytic active components selected from Group IB, IIB, IIIB, IVB, VB, VIB, VIIB and VIIIB elements and catalyst supports selected from Group IIIA, IVA and IVB elements, which were dispersed into inorganic sols (described in Examples 1-7, 12 and 15), organic sols (described in Examples 13 and 14) and inorganic-organic sols (described in Examples 16 and 17), followed by gelation in the presence of condensation agents or crosslinkers to prepare gels with catalysts.
- the moisture-resistant catalyst was obtained after drying and thermal treatment.
- the moisture-resistant catalyst was also prepared using inorganic aerogels (described in Examples 8-12 and 15), organic aerogels (described in Examples 13 and 14) and inorganic-organic aerogels (described in Examples 16 and 17), which are used as supports to immobilize catalytic active components selected from Group IB, IIB, IIIB, IVB, VB, VIB, VIIB and VIIIB elements by conventional impregnation, drying and a thermal treatment processes to prepare the moisture-resistant catalyst.
- the moisture-resistant catalyst was further prepared from metal oxide catalysts (described in Examples 18-21), which are dispersed into inorganic sols (described in Examples 1-7, 12 and 15), organic sols (described in Examples 13 and 14) and inorganic-organic sols (described in Examples 16 and 17), followed by gelation in the presence of condensation agents or crosslinkers to prepare gels with metal oxide catalysts.
- the moisture-resistant catalyst is obtained after drying and thermal treatment.
- Catalytic oxidation reactions were tested, under dry conditions, in a fixed bed reactor fed with synthetic air containing different concentrations of nitrogen-containing compounds.
- the operating temperature was controlled with heating tape, a thermocouple and a thermal controller.
- the metal oxide catalysts and moisture-resistant catalysts were pre-treated in synthetic air at 250° C. for 2 hours.
- the reaction products were analyzed online by a 6890 Series gas chromatograph, manufactured by Agilent®, and equipped with an Alltech® column, manufactured by W. R. Grace & Co., packed with Hayesep® Q 80/100, manufactured by Hayes Separation, Inc., and a thermal conductivity detector.
- Catalytic oxidation reactions were tested, under wet conditions, in a fixed bed reactor fed with synthetic air containing different concentrations of nitrogen-containing compounds and saturated water vapor.
- the operating temperature was controlled with a heating tape, a thermocouple and a thermal controller.
- the metal oxide catalysts and moisture-resistant catalysts were pre-treated in synthetic air at 250° C. for 2 hours.
- the reaction products were analyzed online by a 6890 Series gas chromatograph, manufactured by Agilent®, and equipped with an Alltech® column, manufactured by W. R. Grace & Co., packed with Hayesep® Q 80/100, manufactured by Hayes Separation, Inc., and a thermal conductivity detector.
Abstract
Description
TABLE 1 |
Surface Area and Pore Structure Data for Silica Aerogel, |
Metal Oxide Catalyst and Moisture-Resistant Catalyst |
SBET | VTotal | VMicro | DMeso | |
Sample | (m2/g) | (cm3/g) | (cm3/g) | (nm) |
Silica aerogel | 833.1 | 3.04 | 0.36 | 12.8 |
Metal oxide catalyst | 283.1 | 0.30 | 0.12 | — |
Moisture-resistant catalyst | 685.1 | 2.73 | 0.28 | 7.3 |
Claims (30)
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